Perovskite vacuum drying device

Abstract

The utility model provides a perovskite vacuum drying device. The perovskite vacuum drying device comprises a drying cavity and a placing table arranged in the drying cavity, a sealing plate is arranged on the inner top face of the drying cavity, and an air extraction opening is formed in the surface of the side, perpendicular to the sealing plate, of the drying cavity and used for being externally connected with a vacuumizing device. A plurality of air inlets are formed in the middle of the sealing plate in the air exhaust direction and used for being externally connected with air path guide pipes. A plurality of pipelines are evenly distributed on the side, facing the containing table, of the sealing plate in parallel and correspond to the air inlets. And air outlet holes are uniformly distributed in one side, facing the placing table, of each pipeline. The perovskite vacuum drying device provided by the utility model can control the local area concentration of a volatile solvent in a crystallization process, so that a high-quality perovskite thin film is obtained in each large-size area, accurate control of each crystal orientation is realized, and a large-area perovskite thin film with uniform crystal orientation is obtained.

Description

Technical Field

[0001] The utility model belongs to the technical field of drying devices and relates to a perovskite vacuum drying device. Background Art

[0002] With the rapid development of the photovoltaic industry, the efficiency of N-type silicon solar cell modules has exceeded 24%, approaching the efficiency limit of crystalline silicon cells. Meanwhile, perovskite cells, a new darling of the photovoltaic industry, have emerged as a rising star, with efficiencies exceeding 26%. The efficiency of a single 1000mm*2000mm perovskite module has even exceeded 19%, reaching mass production levels. As the large-scale industrialization of perovskite accelerates, the stability of the perovskite cell fabrication process remains to be determined, as this will limit its competitiveness with traditional crystalline silicon cells in the photovoltaic power station sector. Large-area perovskite films are primarily produced through slit-coating wet coating, and controlling the perovskite crystallization process is paramount in perovskite fabrication.

[0003] Currently, there are two main perovskite crystallization processes: one uses an air knife to blow away the solvent in the perovskite precursor solution, and the other uses vacuum control to volatilize the solvent at the solvent's saturated vapor pressure, i.e., vacuum drying. Because the uniformity of air output from the air knife is difficult to control, vacuum drying is the primary method used for perovskite crystallization in industrialization. Although vacuum drying equipment is widely used in the traditional panel industry, the mass production of perovskites still faces issues such as uncontrollable solvent atmosphere and uneven crystallization. This in turn affects grain growth, defect formation, and mesophase formation during the perovskite crystallization process, ultimately affecting the performance and lifespan of solar cells.

[0004] Existing perovskite vacuum drying equipment mostly uses bottom- or top-exhaust designs, which fail to consider the distribution of volatile solvents during perovskite crystallization and cannot precisely control the perovskite crystal quality in each region during the crystallization process. Therefore, there is an urgent need to design and develop a perovskite vacuum drying device that overcomes the shortcomings of existing technologies and meets practical application needs. Utility Model Content

[0005] In response to the shortcomings of the existing technology, the purpose of the present invention is to provide a perovskite vacuum drying device. In the present invention, through the specific structural design of the perovskite vacuum drying device, the local area concentration of the volatile solvent during the crystallization process can be controlled to achieve high-quality perovskite films in all areas on a large scale, thereby achieving precise control of each crystal orientation, obtaining a large-area perovskite film with uniform crystal orientation, and improving the performance and stability of the component.

[0006] To achieve this purpose, the present invention adopts the following technical solutions:

[0007] The utility model provides a perovskite vacuum drying device, which comprises a drying chamber and a placement table arranged in the drying chamber, wherein the placement table is used to carry a perovskite film;

[0008] A sealing plate is provided on the inner top surface of the drying chamber, and an air extraction port is provided on a side surface of the drying chamber perpendicular to the sealing plate, and the air extraction port is used to connect to an external vacuum device;

[0009] The sealing plate is provided with a plurality of air inlets in the middle along the air extraction direction, the plurality of air inlets are arranged linearly, and the air inlets are used to connect to an external air conduit;

[0010] A plurality of pipelines are evenly distributed in parallel on one side of the sealing plate facing the placement table, and the plurality of pipelines are correspondingly provided with the plurality of air inlets, one end of the air inlet is used to connect to the air source, and the other end is used to connect to the middle of the pipeline;

[0011] Each of the pipelines is evenly distributed with air outlet holes on one side facing the placement table.

[0012] In the present invention, through the specific structural design of the perovskite vacuum drying device, the local area concentration of the volatile solvent during the crystallization process can be controlled to achieve high-quality perovskite films in all areas on a large scale, thereby achieving precise control of each crystal orientation and obtaining a large-area perovskite film with uniform crystal orientation, thereby improving the performance and stability of the component.

[0013] It should be noted that the present invention, through the design of the specific structure of the drying chamber, placement table, sealing plate and side exhaust port combination, can control the local concentration of the volatile solvent during the crystallization process to achieve high-quality perovskite films in all regions on a large scale and precise control of each crystal orientation. A uniform perovskite wet film can be prepared by slit coating and placed in a drying device. The vacuum pump parameters are set in sequence to instantly reduce the pressure of the drying chamber to below the saturated vapor pressure of the perovskite solvent. The air conduit in the sealing plate is then opened to achieve precise ventilation of each pipeline. At the same time, controlling the gas flow in the air conduit at the same pumping speed can also control the cavity pressure of the drying chamber, so that the perovskite film crystallizes at a fixed value below the saturated vapor pressure. The extracted solvent is carried by the gas to achieve precise control of the local concentration, that is, to achieve the effect of inert gas protection to extend the Q-Time of the perovskite wet film, and also to achieve control of the crystal orientation of the perovskite crystals in different regions, ultimately obtaining a large-area perovskite film with uniform crystal orientation, improving component performance and component stability. Among them, Q-Time is the waiting time tracked from one step to the next step. It has a maximum time or a minimum time and refers to the time required between the perovskite wet film processing steps.

[0014] It should be noted that the present invention does not limit the specific dimensions of the drying chamber, the placement table, and the sealing plate, and those skilled in the art may make adaptive adjustments based on actual conditions.

[0015] It should be noted that the function of the gas conduit in the present invention is to pass the gas into the drying chamber; wherein the type of gas can be an inert gas or a perovskite precursor solvent and its anti-solvent, the inert gas is one or more of helium, neon, argon, krypton, xenon, and radon; the perovskite precursor solvent gas is a mixture of one or more of N,N-dimethylformamide, dimethyl sulfoxide, γ-butyrolactone, N-methylpyrrolidone, acetonitrile, ethanol, dimethylacetamide, and 2-mercaptoethanol; the anti-solvent gas of the perovskite precursor solvent is chlorobenzene, acetic acid, One or more mixtures of ethyl ester, methyl benzoate, toluene, dichloromethane, anisole, diethyl carbonate, trifluorobenzene, ethanol, isopropyl alcohol, ethyl benzoate, diethyl carbonate, tetraethoxymethane, dimethyl carbonate, and petroleum ether; and the number of air conduits can be matched with the air inlet. For example, the number of air conduits can be set according to the distance of the longest side of the drying chamber at intervals of 10 to 20 mm, and each air conduit can be independently controlled to ventilate or stop supplying gas, thereby controlling the air flow rate of each air outlet.

[0016] It should be noted that the arrangement of the pipelines in the present invention can be arranged perpendicularly or parallel to the exhaust direction. When the pipelines are arranged perpendicular to the exhaust direction, the number of pipelines can be set according to the distance of the longest side of the drying chamber, which is rounded off by 10 to 20 mm; when the pipelines are arranged parallel to the exhaust direction, the number of pipelines can be set according to the distance of the shortest side of the drying chamber, which is rounded off by 10 to 20 mm.

[0017] It should be noted that the number of air outlets in the present invention is not limited and can be adjusted by those skilled in the art based on actual conditions. Specifically, when the pipes are arranged perpendicular to the direction of air extraction, the number of air outlets can be set according to the distance between the longest side of the drying chamber, rounded up to an integer of 0.1 to 10 mm. When the pipes are arranged parallel to the direction of air extraction, the number of air outlets can be set according to the distance between the shortest side of the drying chamber, rounded up to an integer of 0.1 to 10 mm.

[0018] It should be noted that the “several air inlets” mentioned in the present invention may be, for example, 1, 2, 3, 5, 10, 20, etc., and these are not exhaustive. Those skilled in the art may make adaptive adjustments according to actual conditions.

[0019] It should be noted that the "several pipelines" mentioned in the present invention may be, for example, 1, 2, 3, 5, 10, 20, etc., which are not exhaustive and can be adaptively adjusted by those skilled in the art according to actual conditions. The pipelines may be made of metal.

[0020] As a preferred technical solution of the present invention, the sealing plate is sealed and connected to the drying chamber via a sealing member.

[0021] Preferably, the sealing member is a sealing ring.

[0022] It should be noted that the present invention does not impose any specific restrictions on the specific shape, material and quantity of the sealing ring, and those skilled in the art can make adaptive adjustments based on actual conditions; among them, the material of the sealing ring can be rubber, and the setting method can be to set it in a circle around the circumference of the sealing plate.

[0023] As a preferred technical solution of the present invention, a first vacuum gauge is provided through the sealing plate, and the first vacuum gauge is used to monitor the gas pressure in the drying chamber.

[0024] It should be noted that the model and quantity of the first vacuum gauge in the present invention are not particularly limited. Those skilled in the art can make adaptive adjustments based on actual conditions. All known vacuum gauges can fall within the protection scope of the present invention.

[0025] As a preferred technical solution of the present invention, at least two height adjustment members are provided on one edge of the sealing plate facing away from the placement table, and the height adjustment members are used to adjust the air outlet height of the air outlet.

[0026] It should be noted that the at least two height adjustment members in the present invention may be, for example, 2, 3, 4, 5, 6, etc., and those skilled in the art may adjust the height of the air outlet vents flexibly by designing the height adjustment members, thereby providing greater adaptability to the needs of different products.

[0027] As a preferred technical solution of the present invention, the height adjustment member is an adjusting screw, one end of the adjusting screw is fixedly connected to the sealing plate, and the other end is movably connected to the top surface of the drying chamber.

[0028] It should be noted that the model and number of the adjusting screws in the present invention are not particularly limited. Those skilled in the art can make adaptive adjustments based on actual conditions. All known adjusting screws are within the scope of protection of the present invention. Specifically, when there are multiple adjusting screws, they can be evenly distributed at the edge of the sealing plate to make the height plane more flat. The height range of the adjusting screws, that is, the height of the air outlet from the perovskite film, can be any value between 5 mm and the height of the perovskite wet film surface when the air duct is attached to the sealing plate.

[0029] As a preferred technical solution of the present invention, a gate valve is provided on the other side of the drying chamber relative to the air extraction port, and the gate valve is used to place the perovskite film after opening.

[0030] Preferably, the door valve is sealed and connected to the drying chamber via a sealing ring.

[0031] It should be noted that the present invention does not impose any special restrictions on the specific model of the door valve, and those skilled in the art can make adaptive adjustments based on actual conditions. Specifically, when a product needs to enter the drying chamber, the door valve can be opened to place the product in, and when the product completes the drying process, the door valve can be opened to take the product out.

[0032] As a preferred technical solution of the present invention, the vacuum pumping device includes a vacuum pipeline and a vacuum pump connected in sequence along the direction of the vacuuming.

[0033] It should be noted that the present invention does not impose any special restrictions on the specific models of vacuum pipelines and vacuum pumps, and those skilled in the art can make adaptive adjustments based on actual conditions; all known models of vacuum pipelines and vacuum pumps can fall within the scope of protection of the present invention.

[0034] Preferably, a butterfly valve is provided in the vacuum pipeline near the exhaust port, and a second vacuum gauge is provided on the side of the vacuum pipeline near the vacuum pump, and the second vacuum gauge is used to monitor and control the gas pressure in the vacuum pipeline.

[0035] It should be noted that the present invention does not impose any special restrictions on the specific model of the butterfly valve, and those skilled in the art can make adaptive adjustments based on actual conditions; all known butterfly valve models can fall within the protection scope of the present invention.

[0036] It should be noted that the model and quantity of the second vacuum gauge in the present invention are not particularly limited. Those skilled in the art can make adaptive adjustments based on actual conditions. The second vacuum gauge can be the same as or different from the first vacuum gauge. All known vacuum gauges can fall within the protection scope of the present invention.

[0037] As a preferred technical solution of the present invention, the placement platform includes a placement plane and a plurality of support members evenly distributed at the bottom of the placement plane.

[0038] It should be noted that the placement plane in the present invention should be placed parallel to the inner top wall of the drying chamber to ensure the drying effect of the perovskite film. Its material is not particularly limited, and those skilled in the art can make adaptive adjustments based on actual conditions.

[0039] It should be noted that the “several support members” mentioned in the present invention may be, for example, 1, 2, 3, 5, 10, 20, etc., and these are not exhaustive. Those skilled in the art may make adaptive adjustments according to actual conditions.

[0040] As a preferred technical solution of the present invention, the support member is a PIN needle.

[0041] It should be noted that the PIN pins in this utility model are a metal material used to conduct (transmit) electricity (signals). Specific materials used include polytetrafluoroethylene, polyetheretherketone, and stainless steel. The number of PIN pins can be set according to the distance between the longest and shortest sides of the drying chamber, rounded up to 10-20 mm. Each PIN pin in this utility model is leveled and used to place the perovskite wet film, ensuring that the solvent atmosphere is evenly extracted from the perovskite wet film surface after the equipment is in operation.

[0042] As a preferred technical solution of the present invention, the sealing plate is an MFC sealing plate.

[0043] Preferably, the airway conduit is an MFC airway conduit.

[0044] It should be noted that the MFC sealing plate and the MFC gas conduit in the present invention can be a stainless steel plate and a PTFE gas conduit respectively.

[0045] Compared with the prior art, the beneficial effects of the present invention are:

[0046] In the present invention, through the specific structural design of the perovskite vacuum drying device, the local area concentration of the volatile solvent during the crystallization process can be controlled to achieve high-quality perovskite films in all areas on a large scale, thereby achieving precise control of each crystal orientation and obtaining a large-area perovskite film with uniform crystal orientation, thereby improving the performance and stability of the component. BRIEF DESCRIPTION OF THE DRAWINGS

[0047] Figure 1 A schematic diagram of the overall structure of a perovskite vacuum drying device provided in one embodiment of the present invention;

[0048] Figure 2A schematic top view of the interior of a sealing plate in a perovskite vacuum drying device provided in one embodiment of the present invention;

[0049] Figure 3 A schematic diagram of the internal structure of a perovskite vacuum drying device provided in a specific embodiment of the present invention;

[0050] Figure 4 XRD test graphs of perovskite films after different ventilation modes are used for the air conduits in the perovskite vacuum drying devices provided in Examples 1 and 2;

[0051] Among them, 1-drying chamber; 2-placing plane; 3-PIN needle; 4-air conduit; 5-pipeline; 6-air inlet; 7-air outlet; 8-air extraction port; 9-butterfly valve; 10-gate valve; 11-first vacuum gauge; 12-second vacuum gauge; 13-vacuum pump. DETAILED DESCRIPTION

[0052] It should be understood that, in the description of the present invention, the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, the terms "first", "second", etc. are only used for descriptive purposes, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, features defined as "first", "second", etc. may explicitly or implicitly include one or more of such features. In the description of the present invention, unless otherwise specified, "multiple" means two or more.

[0053] It should be noted that, in the description of this utility model, unless otherwise expressly specified or limited, the terms "disposed," "connected," and "connected" should be understood in a broad sense. For example, they can refer to fixed connections, detachable connections, or integral connections; mechanical connections, electrical connections; direct connections, indirect connections through an intermediate medium, and internal connections between two components. Those skilled in the art will understand the specific meanings of the above terms in this utility model based on specific circumstances.

[0054] The technical solution of the present invention will be further described below with reference to the accompanying drawings and through specific implementation methods.

[0055] In a specific embodiment, the present invention provides a perovskite vacuum drying device, such as Figure 1 、 Figure 2 and Figure 3 As shown, the perovskite vacuum drying device includes a drying chamber 1 and a placement table arranged in the drying chamber 1, and the placement table is used to support the perovskite film;

[0056] A sealing plate is provided on the inner top surface of the drying chamber 1, and an air extraction port 8 is provided on a side surface of the drying chamber 1 perpendicular to the sealing plate. The air extraction port 8 is used to connect to an external vacuum device.

[0057] The middle part of the sealing plate is provided with a plurality of air inlets 6 along the air extraction direction. The plurality of air inlets 6 are arranged linearly and are used to connect to the external air conduit 4.

[0058] A plurality of pipelines 5 are evenly distributed in parallel on one side of the sealing plate facing the placement table. The plurality of pipelines 5 are correspondingly provided with a plurality of air inlets 6. One end of the air inlet 6 is used to connect to the air source, and the other end is used to connect to the middle of the pipeline 5.

[0059] Each pipeline 5 is evenly distributed with air outlet holes 7 on one side facing the placement table.

[0060] In the present invention, through the specific structural design of the perovskite vacuum drying device, the local area concentration of the volatile solvent during the crystallization process can be controlled to achieve high-quality perovskite films in all areas on a large scale, thereby achieving precise control of each crystal orientation and obtaining a large-area perovskite film with uniform crystal orientation, thereby improving the performance and stability of the component.

[0061] It should be noted that the present invention, through the design of the specific structure of the drying chamber 1, the placement table, the sealing plate, and the exhaust port 8 on the side, can control the local concentration of the volatile solvent during the crystallization process to achieve high-quality perovskite films in all regions on a large scale and precise control of each crystal orientation. A uniform perovskite wet film can be prepared by slit coating and placed in a drying device. The vacuum pump 13 parameters are sequentially set to instantly reduce the pressure of the drying chamber 1 to below the saturated vapor pressure of the perovskite solvent. Then, the air conduit 4 in the sealing plate is opened to achieve precise ventilation of each pipeline 5. At the same time, controlling the gas flow in the air conduit 4 at the same pumping speed can also control the cavity pressure of the drying chamber 1, so that the perovskite film crystallizes at a fixed value below the saturated vapor pressure. The extracted solvent is carried by the gas to achieve precise control of the local concentration, that is, to achieve the effect of inert gas protection to extend the Q-Time of the perovskite wet film, and also to achieve control of the crystal orientation of the perovskite crystals in different regions, ultimately obtaining a large-area perovskite film with uniform crystal orientation, improving the performance and stability of the component. Among them, Q-Time is the waiting time tracked from one step to the next step. It has a maximum time or a minimum time and refers to the time required between the perovskite wet film processing steps.

[0062] It should be noted that the present invention does not limit the specific dimensions of the drying chamber 1 , the placement table, and the sealing plate, and those skilled in the art may make adaptive adjustments based on actual conditions.

[0063] It should be noted that the function of the gas conduit 4 in the present invention is to pass the gas into the drying chamber 1; wherein the type of gas can be an inert gas or a perovskite precursor solvent and its anti-solvent, the inert gas is one or more of helium, neon, argon, krypton, xenon, and radon; the perovskite precursor solvent gas is a mixture of one or more of N, N-dimethylformamide, dimethyl sulfoxide, γ-butyrolactone, N-methylpyrrolidone, acetonitrile, ethanol, dimethylacetamide, and 2-mercaptoethanol; the anti-solvent gas of the perovskite precursor solvent is chlorobenzene, ethyl acetate, or the like. , methyl benzoate, toluene, dichloromethane, anisole, diethyl carbonate, trifluorobenzene, ethanol, isopropyl alcohol, ethyl benzoate, diethyl carbonate, tetraethoxymethane, dimethyl carbonate, petroleum ether or a mixture thereof; and the number of the air conduits 4 can be matched with the air inlet 6. For example, the number of the air conduits 4 can be set according to the number of 10 to 20 mm intervals of the longest side of the drying chamber 1. Each air conduit 4 can be independently controlled to ventilate or stop supplying air, thereby controlling the air flow rate of each air outlet 7.

[0064] It should be noted that the arrangement of the pipelines 5 in the present invention can be arranged perpendicularly or parallel to the exhaust direction. When the pipelines 5 are arranged perpendicular to the exhaust direction, the number of pipelines 5 can be set according to the distance of the longest side of the drying chamber 1, which is rounded off by 10 to 20 mm; when the pipelines 5 are arranged parallel to the exhaust direction, the number of pipelines 5 can be set according to the distance of the shortest side of the drying chamber 1, which is rounded off by 10 to 20 mm.

[0065] It should be noted that the number of air outlets 7 in the present invention is not limited and can be adjusted by those skilled in the art based on actual conditions. Specifically, when the pipes 5 are arranged perpendicular to the direction of air extraction, the number of air outlets 7 can be set to the nearest integer of 0.1 to 10 mm between the longest side of the drying chamber 1. When the pipes 5 are arranged parallel to the direction of air extraction, the number of air outlets 7 can be set to the nearest integer of 0.1 to 10 mm between the shortest side of the drying chamber 1.

[0066] It should be noted that the “several air inlets 6” mentioned in the present invention may be, for example, 1, 2, 3, 5, 10, 20, etc., and these are not exhaustive. Those skilled in the art may make adaptive adjustments according to actual conditions.

[0067] It should be noted that the "several pipelines 5" mentioned in the present invention may be, for example, 1, 2, 3, 5, 10, 20, etc., which are not exhaustive and can be adaptively adjusted by those skilled in the art according to actual conditions. The pipeline 5 may be made of metal.

[0068] In one embodiment, the sealing plate is sealed and connected to the drying chamber 1 via a sealing member.

[0069] In one embodiment, the sealing member is a sealing ring.

[0070] It should be noted that the present invention does not impose any specific restrictions on the specific shape, material and quantity of the sealing ring, and those skilled in the art can make adaptive adjustments based on actual conditions; among them, the material of the sealing ring can be rubber, and the setting method can be to set it in a circle around the circumference of the sealing plate.

[0071] In one embodiment, a first vacuum gauge 11 is provided through the sealing plate. The first vacuum gauge 11 is used to monitor the gas pressure in the drying chamber 1 .

[0072] It should be noted that the model and quantity of the first vacuum gauge 11 in the present invention are not particularly limited. Those skilled in the art can make adaptive adjustments according to actual conditions. All known vacuum gauges can fall within the protection scope of the present invention.

[0073] In one embodiment, at least two height adjustment members are provided on one edge of the sealing plate facing away from the placement table, and the height adjustment members are used to adjust the outlet height of the air outlet 7 .

[0074] It should be noted that the at least two height adjustment members in the present invention may be, for example, 2, 3, 4, 5, 6, etc., and those skilled in the art can make adaptive adjustments according to actual conditions. In particular, the present invention can flexibly adjust the outlet height of the air outlet 7 by designing the height adjustment member, which is more adaptable to the needs of different products.

[0075] In one embodiment, the height adjustment member is an adjusting screw, one end of which is fixedly connected to the sealing plate, and the other end of which is movably connected to the top surface of the drying chamber 1 .

[0076] It should be noted that the model and quantity of the adjusting screws in the present invention are not particularly limited. Those skilled in the art can make adaptive adjustments according to actual conditions. All known adjusting screws can fall within the protection scope of the present invention.

[0077] In one embodiment, a gate valve 10 is provided on the other side of the drying chamber 1 relative to the air extraction port 8 , and the gate valve 10 is used to place the perovskite film after it is opened.

[0078] In one embodiment, the gate valve 10 is sealed and connected to the drying chamber 1 via a sealing ring.

[0079] It should be noted that the present invention does not impose any special restrictions on the specific model of the door valve 10, and those skilled in the art can make adaptive adjustments according to actual conditions; among them, when a product needs to enter the drying chamber 1, the door valve 10 can be opened to put the product in, and when the product completes the drying process, the door valve 10 can be opened to take the product out.

[0080] In one embodiment, the vacuum pumping device includes a vacuum pipeline and a vacuum pump 13 connected in sequence along the direction of the vacuuming.

[0081] It should be noted that the present invention does not impose any special restrictions on the specific models of the vacuum pipeline and the vacuum pump 13, and those skilled in the art can make adaptive adjustments based on actual conditions; all known models of vacuum pipelines and vacuum pumps 13 can fall within the protection scope of the present invention.

[0082] In one embodiment, a butterfly valve 9 is provided in the vacuum pipeline near the exhaust port 8, and a second vacuum gauge 12 is provided on the side of the vacuum pipeline near the vacuum pump 13. The second vacuum gauge 12 is used to monitor and control the gas pressure in the vacuum pipeline.

[0083] It should be noted that the present invention does not impose any special restrictions on the specific model of the butterfly valve 9, and those skilled in the art can make adaptive adjustments based on actual conditions; all known models of butterfly valve 9 can fall within the protection scope of the present invention.

[0084] It should be noted that the model and quantity of the second vacuum gauge 12 in the present invention are not particularly limited. Those skilled in the art can make adaptive adjustments according to actual conditions. The second vacuum gauge 12 can be the same as or different from the first vacuum gauge 11. All known vacuum gauges can fall within the protection scope of the present invention.

[0085] In one embodiment, the placement platform includes a placement plane 2 and a plurality of support members evenly distributed at the bottom of the placement plane 2 .

[0086] It should be noted that the placement plane 2 in the present invention should be placed parallel to the inner top wall of the drying chamber 1 to ensure the drying effect of the perovskite film. Its material is not particularly limited, and those skilled in the art can make adaptive adjustments according to actual conditions.

[0087] It should be noted that the “several support members” mentioned in the present invention may be, for example, 1, 2, 3, 5, 10, 20, etc., and these are not exhaustive. Those skilled in the art may make adaptive adjustments according to actual conditions.

[0088] In one embodiment, the support member is a PIN needle 3 .

[0089] It should be noted that the PIN pins 3 in the present invention are a metal material used to conduct (transmit) electricity (signals). Specific materials used include polytetrafluoroethylene, polyetheretherketone, and stainless steel. The number of PIN pins 3 can be set to the nearest integer of 10 to 20 mm, based on the distance between the longest and shortest sides of the drying chamber 1. Each PIN pin 3 in the present invention is leveled and used to place the perovskite wet film, ensuring that the solvent atmosphere is evenly removed from the perovskite wet film surface after the device is in operation.

[0090] In one embodiment, the sealing plate is an MFC sealing plate.

[0091] In one embodiment, the airway conduit 4 is an MFC airway conduit 4 .

[0092] It should be noted that the MFC sealing plate and the MFC gas conduit 4 in the present invention can be a stainless steel plate and a PTFE gas conduit 4 respectively.

[0093] Exemplarily, the control method of the perovskite vacuum drying device in the present invention is as follows:

[0094] S1: Close the butterfly valve 9, set the pressure of the vacuum pump 13, i.e. the pressure of the second vacuum gauge 12, to 0.1-100 Pa, start the vacuum pump 13 and pump the pressure of the pipeline 5 to the set value;

[0095] S2: Open the door panel, place the perovskite wet film obtained after slit coating into the drying chamber 1, and close the door panel valve 10;

[0096] S3: Adjust the height adjustment screw so that the lowest point of pipe 5 is 1 to 10 cm away from the surface of the perovskite wet film;

[0097] S4: Open each gas conduit 4 and set the gas flow rate of the gas to 500-50000 sccm;

[0098] S5: Open the butterfly valve 9 to quickly reduce the pressure in the drying chamber 1 to 20-50 Pa within 10 seconds;

[0099] S6: vacuum pump 13 maintains pressure for 10 to 80 seconds;

[0100] S7: Close the butterfly valve 9, open the gate valve 10, and after the drying chamber 1 returns to normal pressure, take out the product and proceed with the subsequent perovskite preparation process to complete the component preparation.

[0101] It should be noted that, in the present invention, sccm refers to the flow rate under standard conditions (ie, 1 atmospheric pressure, 25 degrees Celsius, 1 cubic centimeter per minute); normal pressure is 1 atmospheric pressure.

[0102] Among them, half of the gas conduits 4 in S4 can be filled with N,N-dimethylformamide gas, and the other half can be filled with nitrogen gas, and the flow rate and content of the two are consistent. This is because passing nitrogen through all the gas conduits 4 may cause excessive local nitrogen concentration and uneven crystallization; it is also possible that nitrogen is passed through the odd-numbered gas conduits 4 in S4, and N,N-dimethylformamide gas is passed through the even-numbered gas conduits 4, so that the flow rate of nitrogen is 1 to 2 times the flow rate of N,N-dimethylformamide gas. This setting is because there is a flow direction of gas during vacuum drying, and the concentration of the solvent formed by drying on the surface of the film is controlled by passing the perovskite solvent and nitrogen at intervals, which plays a role in uniform crystallization; at the same time, passing the perovskite solvent can also control the crystallization rate of the perovskite film and expand the perovskite precursor window.

[0103] Example 1

[0104] This embodiment provides a perovskite vacuum drying device, wherein:

[0105] The perovskite vacuum drying device includes a drying chamber 1 and a placement table arranged in the drying chamber 1, which is used to carry the perovskite film; an MFC sealing plate is provided on the inner top surface of the drying chamber 1, and an exhaust port 8 is provided on the side surface of the drying chamber 1 perpendicular to the MFC sealing plate, and the exhaust port 8 is used to connect to an external vacuum device; a plurality of air inlets 6 are provided in the middle of the MFC sealing plate along the exhaust direction, and the plurality of air inlets 6 are arranged linearly, and the air inlets 6 are used to connect to an external MFC air path duct 4; a plurality of pipelines 5 are evenly distributed in parallel on the side of the MFC sealing plate facing the placement table, and the plurality of pipelines 5 and the plurality of air inlets 6 are correspondingly arranged, one end of the air inlet 6 is used to connect to the air source, and the other end is used to connect to the middle of the pipeline 5; each pipeline 5 is evenly distributed with an air outlet 7 on the side facing the placement table.

[0106] The MFC sealing plate is sealed and connected to the drying chamber 1 through a sealing ring. A first vacuum gauge 11 is provided through the MFC sealing plate. Four adjusting screws are provided on the edge of the MFC sealing plate facing away from the placement table. One end of the adjusting screw is fixedly connected to the MFC sealing plate, and the other end is movably connected to the top surface of the drying chamber 1.

[0107] A gate valve 10 is provided on the other side of the drying chamber 1 opposite to the air extraction port 8 , and the gate valve 10 is sealedly connected to the drying chamber 1 via a sealing ring.

[0108] The vacuum pumping device includes a vacuum pipeline and a vacuum pump 13 connected in sequence along the direction of the vacuuming. A butterfly valve 9 is provided in the vacuum pipeline near the vacuum port 8, and a second vacuum gauge 12 is provided on the side of the vacuum pipeline near the vacuum pump 13.

[0109] The placement platform includes a placement plane 2 and a plurality of PIN needles 3 evenly distributed on the bottom of the placement plane 2 .

[0110] When using this perovskite vacuum drying device, all the MFC gas conduits 4 are ventilated.

[0111] According to the XRD analysis of the fully opened MFC gas conduit 4, there are problems with the crystal orientation of some areas. Precise ventilation is performed in this area to achieve a wind knife-like effect in the local area to control the crystal orientation of the seed crystal, and finally a perovskite film with consistent XRD (crystallization orientation) is obtained.

[0112] Example 2

[0113] This embodiment provides a perovskite vacuum drying device, wherein:

[0114] The perovskite vacuum drying device includes a drying chamber 1 and a placement table arranged in the drying chamber 1, which is used to carry the perovskite film; an MFC sealing plate is provided on the inner top surface of the drying chamber 1, and an exhaust port 8 is provided on the side surface of the drying chamber 1 perpendicular to the MFC sealing plate, and the exhaust port 8 is used to connect to an external vacuum device; a plurality of air inlets 6 are provided in the middle of the MFC sealing plate along the exhaust direction, and the plurality of air inlets 6 are arranged linearly, and the air inlets 6 are used to connect to an external MFC air path duct 4; a plurality of pipelines 5 are evenly distributed in parallel on the side of the MFC sealing plate facing the placement table, and the plurality of pipelines 5 and the plurality of air inlets 6 are correspondingly arranged, one end of the air inlet 6 is used to connect to the air source, and the other end is used to connect to the middle of the pipeline 5; each pipeline 5 is evenly distributed with an air outlet 7 on the side facing the placement table.

[0115] The MFC sealing plate is sealed and connected to the drying chamber 1 through a sealing ring. A first vacuum gauge 11 is provided through the MFC sealing plate. Four adjusting screws are provided on the edge of the MFC sealing plate facing away from the placement table. One end of the adjusting screw is fixedly connected to the MFC sealing plate, and the other end is movably connected to the top surface of the drying chamber 1.

[0116] A gate valve 10 is provided on the other side of the drying chamber 1 opposite to the air extraction port 8 , and the gate valve 10 is sealedly connected to the drying chamber 1 via a sealing ring.

[0117] The vacuum pumping device includes a vacuum pipeline and a vacuum pump 13 connected in sequence along the direction of the vacuuming. A butterfly valve 9 is provided in the vacuum pipeline near the vacuum port 8, and a second vacuum gauge 12 is provided on the side of the vacuum pipeline near the vacuum pump 13.

[0118] The placement platform includes a placement plane 2 and a plurality of PIN needles 3 evenly distributed on the bottom of the placement plane 2 .

[0119] When using the perovskite vacuum drying device, every other MFC gas conduit 4 is ventilated.

[0120] exist Figure 4The XRD graph is the XRD curve of the film closest to the air duct 4. The control group is the XRD curve after all the air ducts 4 are opened in Example 1, and the experimental group is the XRD curve after ventilation is performed with one duct left. In the figure, the peak intensity at 13.8° corresponds to the 100° position of the perovskite crystal phase. It can be seen that the crystallization peak intensity of the experimental group is significantly higher and the half-peak width is smaller. At the same time, 100° as the main crystal phase represents that the experimental group has a very good crystal orientation, which also proves the feasibility of the technical solution in the present invention.

[0121] In summary, the utility model, through the specific structural design of the perovskite vacuum drying device, can control the local area concentration of the volatile solvent during the crystallization process to obtain high-quality perovskite films in all areas on a large scale, thereby achieving precise control of each crystal orientation, and obtaining a large-area perovskite film with uniform crystal orientation, thereby improving the performance and stability of the component.

[0122] The above description is only a specific implementation method of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed in the present invention fall within the protection scope and disclosure scope of the present invention.

Claims

1. A perovskite vacuum drying device, characterized in that: The perovskite vacuum drying device includes a drying chamber and a placement table arranged in the drying chamber, wherein the placement table is used to support the perovskite film; A sealing plate is provided on the inner top surface of the drying chamber, and an air extraction port is provided on a side surface of the drying chamber perpendicular to the sealing plate, and the air extraction port is used to connect to an external vacuum device; The sealing plate is provided with a plurality of air inlets in the middle along the air extraction direction, the plurality of air inlets are arranged linearly, and the air inlets are used to connect to an external air conduit; A plurality of pipelines are evenly distributed in parallel on one side of the sealing plate facing the placement table, and the plurality of pipelines are correspondingly provided with the plurality of air inlets, one end of the air inlet is used to connect to the air source, and the other end is used to connect to the middle of the pipeline; Each of the pipelines is evenly distributed with air outlet holes on one side facing the placement table.

2. The perovskite vacuum drying device according to claim 1, characterized in that The sealing plate is sealed and connected to the drying chamber via a sealing member; The sealing member is a sealing ring.

3. The perovskite vacuum drying device according to claim 1, characterized in that A first vacuum gauge is provided through the sealing plate, and the first vacuum gauge is used to monitor the gas pressure in the drying chamber.

4. The perovskite vacuum drying device according to claim 1, characterized in that At least two height adjustment members are provided on one side edge of the sealing plate facing away from the placement table, and the height adjustment members are used to adjust the air outlet height of the air outlet holes.

5. The perovskite vacuum drying device according to claim 4, characterized in that: The height adjustment member is an adjustment screw, one end of which is fixedly connected to the sealing plate, and the other end of which is movably connected to the inner top surface of the drying chamber.

6. The perovskite vacuum drying device according to claim 1, characterized in that: A gate valve is provided on the other side of the drying chamber relative to the air extraction port, and the gate valve is used to place the perovskite film after opening; The door plate valve is sealed and connected to the drying chamber via a sealing ring.

7. The perovskite vacuum drying device according to claim 1, characterized in that: The vacuum pumping device includes a vacuum pipeline and a vacuum pump connected in sequence along the direction of the vacuuming; A butterfly valve is provided in the vacuum pipeline near the air extraction port, and a second vacuum gauge is provided on the side of the vacuum pipeline near the vacuum pump, and the second vacuum gauge is used to monitor and control the gas pressure in the vacuum pipeline.

8. The perovskite vacuum drying device according to claim 1, characterized in that: The placement platform includes a placement plane and a plurality of support members evenly distributed at the bottom of the placement plane.

9. The perovskite vacuum drying device according to claim 8, characterized in that: The supporting member is a PIN needle.

10. The perovskite vacuum drying device according to claim 1, characterized in that: The sealing plate is an MFC sealing plate; The airway conduit is an MFC airway conduit.

Images